EP2808313B1 - Corps fritté d'alumine colorée à haute ténacité et translucidité élevée, son procédé de production et ses utilisations - Google Patents

Corps fritté d'alumine colorée à haute ténacité et translucidité élevée, son procédé de production et ses utilisations Download PDF

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Publication number
EP2808313B1
EP2808313B1 EP14173391.5A EP14173391A EP2808313B1 EP 2808313 B1 EP2808313 B1 EP 2808313B1 EP 14173391 A EP14173391 A EP 14173391A EP 2808313 B1 EP2808313 B1 EP 2808313B1
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Prior art keywords
group
metal oxides
sintered body
alumina
total
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EP14173391.5A
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German (de)
English (en)
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EP2808313A2 (fr
EP2808313A3 (fr
Inventor
Isao Yamashita
Koji Tsukuma
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Tosoh Corp
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Tosoh Corp
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Priority claimed from JP2008294499A external-priority patent/JP5458553B2/ja
Priority claimed from JP2008294498A external-priority patent/JP5458552B2/ja
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Publication of EP2808313A3 publication Critical patent/EP2808313A3/fr
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
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    • C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9646—Optical properties
    • C04B2235/9661—Colour

Definitions

  • the present invention relates to a colored alumina sintered body having both high toughness and excellent translucency, which is not only useful in ornament, jewelry and craftwork articles, but available as dental materials such as an orthodontic bracket and a mill blank for artificial denture which require high value in toughness.
  • a translucent alumina sintered body has been widely utilized not only in ornament, jewelry and craftwork articles, but as dental materials such as an orthodontic bracket and a mill blank for artificial denture.
  • dental materials such as an orthodontic bracket and a mill blank for artificial denture.
  • the improvement of mechanical properties such as fracture toughness in addition to aesthetic nature based on translucency become an important issue in the translucent alumina sintered body.
  • the enhancement in toughness of a translucent alumina sintered body characterized by coloring hereinafter, translucent colored alumina sintered body
  • Patent documents 1-6 disclose a method of mixing an alumina powder with cobalt oxide, nickel oxide, chromium oxide, manganese oxide, and so on, and sintering the mixture under hydrogen or vacuum atmosphere.
  • Patent document 2 discloses a method for producing a translucent colored alumina sintered body by a hot isostatic pressing (HIP) using transition metals such as iron oxide, titanium oxide, vanadium oxide, nickel oxide, chromium oxide and cobalt oxide. Using these methods, translucent colored alumina sintered bodies having color such as blue, green, yellow and pink are obtained.
  • HIP hot isostatic pressing
  • Patent document 9 Regarding the enhancement in toughness of an alumina sintered body, there are reports such as the introduction of different phases (Patent document 9, and Non-Patent document 1) and the anisotropic grain growth of alumina grains (Patent documents 10 and 11). Using these methods, high value in fracture toughness is obtained, but translucency does not appear. The reason for this is considered that the introduction of different phases causes light scattering at interfaces of different phases, and also a sintered body texture containing anisotropic grains, which can be formed by said conventional method, lowers translucency (Patent document 12).
  • Patent document D13 describes a sintered alumina ceramic containing 1 wt% of titania and 2 wt% of magnesia as additives.
  • the ceramic was sintered pressureless at 1500°C and then HIPped at 1400°C.
  • the toughness was 4.8 MPa.m 0.5 .
  • Non-Patent document 2 describes a sintered alumina ceramic containing 0-0.4 wt% of manganese oxide as additive.
  • the ceramic was sintered pressureless at 1200-1400°C.
  • the total transmittance of a 0.5 mm thick sample with 0.05 wt% MnO that was sintered pressureless at 1250°C and then HIPped at 1400°C with 100 MPa was higher than 70%.
  • the present invention relates to providing a colored alumina sintered body having both high toughness and translucency, and a method for producing the same.
  • the gist of the present invention resides in the following (1)-(5).
  • a conventional translucent colored alumina sintered body had low toughness, destroyed during processing, and lacked impact-resistance when applying stress.
  • the alumina sintered body of the present invention has coloring with high aesthetic nature and translucency, as well as higher toughness than that of the conventional sintered body, and thus it has excellent processability, and does not destroy or break.
  • An alumina sintered body of the present invention contains transition metal oxides.
  • a transparent alumina sintered body having the intended color can be obtained.
  • a content of the transition metal oxide is 100ppm-3wt%, and preferably 300ppm-1wt%. If the content is less than 100ppm, an effect of adding the transition metal oxide is liable to be poor, and if the content exceeds 3wt%, the transition metal oxide in alumina reachs a limit of solid solution, and consequently grains of transition metal oxide are precipitated in the sintered body, and translucency is liable to be lowered.
  • fracture toughness is 4.5 MPa ⁇ m 0.5 or more, particularly preferably 5 MPa ⁇ m 0.5 or more, and more preferably 6 MPa ⁇ m 0.5 or more.
  • the sintered body of the present invention has high translucency, wherein the maximum value of total forward transmittance of a sample having a thickness of 1mm to a light having a wavelength of 300-800nm is 60% or more, 65% or more, particularly preferably 70% or more, and more preferably 75% or more.
  • flexural strength is not particularly limited, but it is preferably 350 MPa or more, particularly preferably 400MPa or more, and more preferably 500MPa or more.
  • Methods for evaluating fracture toughness and flexural strength herein are based on methods defined in JIS, and all values in the present invention are average values (average fracture toughness and average flexural strength).
  • the alumina sintered body of the present invention contains anisotropic grains having a long axis length of 10 ⁇ m or greater and an aspect ratio of 1.5 or more as sintered grains.
  • the aspect ratio of anisotropic grains is preferably 3 or more. The greater the aspect ratio of anisotropec grains, the higher the fracture toughness.
  • a representative example of alumina sintered grains constituting the alumina sintered body is shown in Fig. 1 .
  • a content of anisotropic grains in the alumina sintered body of the present invention is 20vol% or more, preferably 30vol%, and more preferably 50vol% or more.
  • anisotropic grains in the alumina sintered body of the present invention are particularly plate-shaped grains (anisotropic plate-shaped grains).
  • a sintered texture of the alumina sintered body of the present invention comprises equi-axis grains in addition to anisotropic grains, and anisotropic grains contribute to the enhancement of fracture toughness, while equi-axis grains help to interconnect anisotropic grains to contribute to the maintenance of strength.
  • the alumina sintered body of the present invention has high toughness and translucency by virtue of the sintered texture containing specific anisotropic grains, and is different from conventional sintered bodies having low toughness containing aids such as magnesium oxide.
  • the transition metal oxide contained in an alumina sintered body of the present invention may be transition metal oxides having a eutectic point with alumina, and preferably at least one selected from the group consisting of manganese oxide, copper oxide, vanadium oxide, iron oxide, titanium oxide, and nickel oxide. These transition metal oxides not only impart the intended color, but also provide liquid phase in alumina, resulting in promoting anisotropic grain growth of alumina grains.
  • the alumina sintered body of the present invention contains additionally at least one selected from the group consisting of Group 1A alkali metal oxides, Group 2A alkaline earth metal oxides, and SiO 2 , B 2 O 3 , P 2 O 5 and GeO 2 in the range of 20-1000ppm in total, in addition to the transition metal oxide.
  • Group 1A alkali metal oxides such as Na 2 O, Group 2A alkaline earth metal oxides, and SiO 2 , B 2 O 3 , P 2 O 5 and GeO 2 act as a glass forming aid to promote anisotropic grain growth of alumina grains.
  • the oxides having high glass-forming ability are particularly Na 2 O, and Na 2 O + SiO 2 .
  • examples of Group 1A alkali metals of Periodic Table include lithium, sodium, potassium, rubidium and cesium.
  • MgO belongs to Group 2A alkaline earth metal oxides, but MgO shows an effect of acting as a grain growth inhibitor. Therefore, when MgO is used as Group 2A alkaline earth metal oxides, one or more components from the group consisting of Group 1A alkali metal oxides, SiO 2 , B 2 O 3 , P 2 O 5 , GeO 2 and Group 2A alkaline earth metal oxides other than MgO must be added additionally. Therefore, it is preferred that Group 2A alkaline earth metal oxides other than MgO are used.
  • examples of Group 2A alkaline earth metals of Periodic Table include beryllium, magnesium, calcium, strontium and barium.
  • a content of one or more components selected additionally from the group consisting of Group 1A alkali metal oxides, SiO 2 , B 2 O 3 , P 2 O 5 , GeO 2 and Group 2A alkaline earth metal oxides other than MgO contained in the alumina sintered body of the present invention is preferably 20-1000ppm in total. If the content is less than 20ppm, an effect of adding it may be poor, and if the content exceeds 1000ppm, sintering may be inhibited.
  • rare earth metal oxides such as erbium oxide and europium oxide have an effect of coloring an alumina sintered body.
  • the alumina sintered body of the present invention contains at least one selected from the group consisting of Group 1A alkali metal oxides, Group 2A alkaline earth metal oxides, and SiO 2 , B 2 O 3 , P 2 O 5 and GeO 2 in the range of 20-1000ppm in total, and thus the transition metal oxide used is not particularly limited so long as the intended color is colored. For example, cobalt oxide appearing blue, chromium oxide appearing red and the like may be used.
  • a sintered body of the present invention can be produced by molding an alumina powder containing transition metal oxides in the range of 100 ppm-3wt% in total, pressureless sintering the resulting molded article, and subjecting the resulting sintered body to a hot isostatic pressing (HIP) treatment.
  • HIP hot isostatic pressing
  • the transition metal oxide may be transition metal oxides having a eutectic point with alumina, and preferably at least one selected from the group consisting of manganese oxide, copper oxide, vanadium oxide, iron oxide, titanium oxide, and nickel oxide.
  • the alumina powder contains additionally at least one selected from the group consisting of Group 1A alkali metal oxides, Group 2A alkaline earth metal oxides, and SiO 2 , B 2 O 3 , P 2 O 5 and GeO 2 in the range of 20-1000ppm in total, in addition to the transition metal oxide. These oxides promote anisotropic grain growth of alumina grains. For this reason, when containing such oxides, the type of transition metal oxide contained in the alumina powder is not limited, any transition metal oxide appearing the intended color may be used.
  • the alumina powder as a raw material in which said different types of components are added is a high purity alumina powder having purity of 99.99% or more, and it is preferred that the alumina powder includes fine grains having a specific surface area of 5-20m 2 /g, wherein the fraction of 1 ⁇ m or smaller fine grains is 90vol% or more.
  • the high purity alumina powder as a starting raw material, a content of different types of components become uniform, resulting in obtaining a high quality sintered body.
  • the fraction of fine grains in the alumina powder is important, and it is not preferred that the fraction of fine grains is less than 90%, since a temperature for achieving densification by sintering is raised in such a case.
  • said different types of components are added in the alumina powder, and the mixture may be preferably dispersed by a mixing and/or grinding apparatus.
  • a method for mixing and/or grinding the mixture may be a wet method using water, ethanol and the like, or a dry method.
  • oxides may be added as oxide powders, or precursors (chlorides, inorganic acid salts, organic acid salts and the like) which become oxides by a firing process. Furthermore, in case of alkali metal oxides, water-soluble salts such as NaCl may be used. These raw materials are mixed so as to satisfy predetermined amounts, and the resulting mixture may be dried and/or sintered.
  • a method for molding the powder is not particularly limited, and various methods such as mold press, rubber press, slip casting, and injection molding may be applied, for example.
  • a hot isostatic pressing (HIP) treatment is conducted.
  • pressureless sintering is conducted at a temperature of 1250-1450°C preferably under the atmosphere of air, oxygen, vacuum or the like.
  • the pressureless sintering densifies a sintered body to density (about 95% of theoretical density) required for subsequent HIP treatment. If the density after pressureless sintering is less than 95% of theoretical density, pores cannot be removed by the penetration of a pressure medium gas for HIP treatment within the sintered body.
  • pressureless sintering It is preferred in pressureless sintering that residual pores within the sintered body have a form which can be removed effectively by HIP treatment, and particularly intergranular pores may be easily removed relative to intragranular pores. Therefore, if the sintering temperature of pressureless sintering is too high, the phenomenon that pores enter grains by grain growth may be easily generated, and it is difficult to remove such pores by HIP treatment. Furthermore, the more the crystalline grains of a primary sintered body applied to HIP treatment is fine, the more the translucency of sintered body after HIP treatment is increased. Thus, from standpoints of obtaining 95% or more of theoretical density, inhibiting the generation of intragranular pores, and obtaining fine crystalline grains, pressureless sintering is conducted at a temperature of 1250-1450°C.
  • HIP treatment is conducted to remove residual pores within a sintered body and impart translucency thereto.
  • a treatment temperature is of 1450-1650°C, for 1 hour and a treatment pressure is 150MPa. If the temperature is less than 1200°C, the growth of anisotropic grains is insufficient, and if the temperature exceeds 1800°C, anisotropic grains become coarse, and consequently it may be difficult to achieve the effect of the present invention.
  • argon gas As a pressure medium in HIP treatment, argon gas is used.
  • composition and treatment condition of the present invention since forming of anisotropic grains is initiated at a high temperature, densification is achieved without generating intragranular pores which inhibit translucency by densifying fine sintered grains in pressureless sintering. Furthermore, by promoting the growth of anisotropic grains characteristic of the sintered body of the present invention in the subsequent HIP treatment, an alumina sintered body having coloring with high aesthetic nature and high toughness while maintaining high translucency is obtained.
  • a fracture toughness test was measured by SEPB method based on "Fracture toughness test method of fine ceramics" of JIS R1607. An average value of five measurements was adopted.
  • a flexural test was measured by a three-point flexural test based on "Flexural strength test method of fine ceramics" of JIS R1601. An average value of ten measurements was adopted.
  • Total forward transmittance was measured by a double beam-system spectrophotometer (V-650 Model, manufactured by JASCO Corporation) based on "Test method of optical characteristics of plastics" of JIS K7105 and "Test method of total forward transmittance of plastics and transparent materials” of JIS K7361-1.
  • Light emitted from a light source deuterium lamp and halogen lamp
  • a measurement wavelength region was from 200-800nm, and total forward transmittance in the present invention was the maximum value at a wavelength of 300-800nm.
  • a sintered body was mirror-polished, followed by chemical etching to emphasize grain boundaries and coat with gold thereon. It was observed using a scanning electron micrography or optical micrography, and values were calculated by image analysis of these photographs. Each grain approximated to rectangular, and a long side was measured as a long axis length, and a short side was measured as a short axis length. A value obtained by dividing the long axis length by the short axis length was adopted as an aspect ratio. Grains having a long axis length of 10 ⁇ m or greater, and an aspect ratio of 1.5 or more were selected, and volume fraction was calculated from the area occupied by these grains. The number of grains measured was 100 or more.
  • the chemical etching was conducted by immersing a sintered body in a supersaturated sodium borate solution at 80°C to deposit it on a surface of the sintered body, heating at 900°C for 0.5 hour, cooling, and washing using a hydrochloric acid solution.
  • the content of each of transition metal oxides was 500ppm with respect to alumina. Impurities containing in the high purity alumina powder used as the raw material were shown in Table 1. The total amount of these oxides was 20ppm or less. Meanwhile, impurities not shown in Table 1 were not greater than detection limit ( ⁇ 1ppm).
  • cobalt oxide (CoO: manufactured by RARE METALLIC Co., Ltd., 99.9% purity)
  • chromium oxide Cr 2 O 3 : manufactured by RARE METALLIC Co., Ltd., 99.99% purity
  • manganese oxide, vanadium oxide, nickel oxide and sodium metasilicate Na 2 O ⁇ SiO 2 , manufactured by ALDRICH CORPORATION
  • the resulting mixture was dried and used as a raw material powder.
  • the content of each transition metal oxide and sodium metasilicate was 500ppm and 50ppm with respect to alumina, respectively.
  • Sintered bodies were obtained by conducting the same treatment as Example 1 except for using powders having compositions shown in Table 3.
  • the fraction of anisotropic grains having a long axis length of 10 ⁇ m or greater and an aspect ratio of 1.5 or more, fracture toughness, flexural strength, and total forward transmittance of the resulting sintered bodies were determined. The results are shown in Table 3.
  • the translucent colored alumina sintered body of the present invention has both high toughness and translucency, and thus it is very suitable for conventional ornament, jewelry and craftwork articles, as well as dental materials such as an orthodontic bracket and a mill blank for artificial denture which require high toughness not to break upon processing and coloring aesthetic nature for fashion. Therefore, this invention has a significant industrial value.

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Claims (7)

  1. Corps fritté en alumine, caractérisé en ce que le corps fritté en alumine contient des oxydes de métal de transition à raison de 100 ppm à 3 % en poids au total, et contient en outre au moins l'un choisi dans l'ensemble constitué par les oxydes de métal alcalin du Groupe 1A, les oxydes de métal alcalino-terreux du Groupe 2A, et SiO2, B2O3, P2O5 et GeO2 à raison de 20 à 1000 ppm au total, et lorsque le MgO est utilisé en tant qu'oxyde de métal alcalino-terreux du Groupe 2A, un ou plusieurs composants de l'ensemble constitué par les oxydes de métal alcalin du Groupe 1A, SiO2, B2O3, P2O5, GeO2 et les oxydes de métal alcalino-terreux du Groupe 2A autres que le MgO doivent être ajoutés en plus, la ténacité à la fracture est de 4,5 MPa•m0,5 ou plus, et la valeur maximale du coefficient de transmission vers l'avant d'un échantillon ayant une épaisseur de 1 mm vis-à-vis d'une lumière ayant une longueur d'onde de 300 à 800 nm est de 60 % ou plus, les grains frittés comprennent des grains anisotropiques ayant une longueur de l'axe long de 10 µm ou plus, et un rapport d'aspect de 1,5 ou plus, et la fraction des grains anisotropiques ayant une longueur de l'axe long de 10 µm ou plus, et un rapport d'aspect de 1,5 ou plus est de 20 % en volume ou plus.
  2. Corps fritté en alumine selon la revendication 1, caractérisé en ce que le corps fritté en alumine contient au moins l'un choisi dans l'ensemble constitué par les oxydes de métal alcalin du Groupe 1A, les oxydes de métal alcalino-terreux du Groupe 2A autres que MgO, et SiO2, B2O3, P2O5 et GeO2 à raison de 20 à 1000 ppm au total.
  3. Procédé pour produire un corps fritté en alumine tel que défini dans la revendication 1, caractérisé par
    le moulage d'une poudre d'alumine qui est une poudre d'alumine de haute pureté ayant une pureté de 99,99 % ou plus, à laquelle ont été ajoutés des oxydes de métal de transition à raison de 100 ppm à 3 % en poids au total et au moins l'un choisi dans l'ensemble constitué par les oxydes de métal alcalin du Groupe 1A, les oxydes de métal alcalino-terreux du Groupe 2A, et SiO2, B2O3, P2O5 et GeO2 à raison de 20 à 1000 ppm au total, et lorsque le MgO est utilisé en tant qu'oxyde de métal alcalino-terreux du Groupe 2A, un ou plusieurs composants de l'ensemble constitué par les oxydes de métal alcalin du Groupe 1A, SiO2, B2O3, P2O5, GeO2 et les oxydes de métal alcalino-terreux du Groupe 2A autres que le MgO doivent être ajoutés en plus,
    le frittage sans pression de l'article moulé résultant à une température de 1250 à 1450 °C, et
    la soumission du corps fritté résultant à un traitement de pressage isostatique à chaud (HIP) à une température de 1450 à 1650 °C sous une pression de 150 MPa pendant 1 heure dans un milieu d'argon gazeux.
  4. Procédé pour produire un corps fritté en alumine tel que défini dans la revendication 2, caractérisé par
    le moulage d'une poudre d'alumine qui est une poudre d'alumine de haute pureté ayant une pureté de 99,99 % ou plus, à laquelle ont été ajoutés des oxydes de métal de transition à raison de 100 ppm à 3 % en poids au total et au moins l'un choisi dans l'ensemble constitué par les oxydes de métal alcalin du Groupe 1A, les oxydes de métal alcalino-terreux du Groupe 2A autres que MgO, et SiO2, B2O3, P2O5 et GeO2 à raison de 20 à 1000 ppm au total,
    le frittage sans pression de l'article moulé résultant à une température de 1250 à 1450 °C, et
    la soumission du corps fritté résultant à un traitement de pressage isostatique à chaud (HIP) à une température de 1450 à 1650 °C sous une pression de 150 MPa pendant 1 heure dans un milieu d'argon gazeux.
  5. Procédé de production selon la revendication 3 ou 4, caractérisé par l'utilisation d'une poudre d'alumine de haute pureté ayant une surface spécifique de 5 à 20 m2/g, et une fraction de grains fins de 1 µm ou moins de 90 % en volume ou plus.
  6. Matériau à usage dentaire, caractérisé par l'utilisation du corps fritté en alumine selon la revendication 1 ou 2.
  7. Matériau dentaire selon la revendication 6, dans lequel le matériau dentaire est un bracket orthodontique ou une ébauche à fraiser pour prothèse dentaire.
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US8481439B2 (en) 2013-07-09
US20110189622A1 (en) 2011-08-04
EP2366675B1 (fr) 2015-05-27
EP2808313A2 (fr) 2014-12-03
EP2366675A4 (fr) 2013-04-24
WO2010058745A1 (fr) 2010-05-27
EP2808313A3 (fr) 2015-02-25
EP2366675A1 (fr) 2011-09-21

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